CN115779983A - Ion exchange technology-based traditional Chinese medicine decoction potassium removal process - Google Patents
Ion exchange technology-based traditional Chinese medicine decoction potassium removal process Download PDFInfo
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- CN115779983A CN115779983A CN202211299871.9A CN202211299871A CN115779983A CN 115779983 A CN115779983 A CN 115779983A CN 202211299871 A CN202211299871 A CN 202211299871A CN 115779983 A CN115779983 A CN 115779983A
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- potassium
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Abstract
The invention provides a traditional Chinese medicine decoction potassium removal process based on an ion exchange technology, which is characterized in that exchange resins with different masses are added into a traditional Chinese medicine decoction to be subjected to potassium removal exchange at different exchange temperatures and for different exchange action times.
Description
Technical Field
The invention relates to the field of application of potassium ions in traditional Chinese medicine decoction, in particular to a traditional Chinese medicine decoction potassium removal process based on an ion exchange technology.
Background
Potassium ion (K) + ) Is an important cation for maintaining physiological function of human body, and has potassium content of about 150g, about 98% of K + Present in the intracellular fluid and 2% in the extracellular fluid (blood, interstitial fluid). Hyperkalemia can be caused when excessive potassium intake, disturbance of distribution inside and outside cells or abnormal excretion occur due to diet, drugs (such as renin-angiotensin-aldosterone system inhibitor, chinese medicine) or diseases (such as chronic kidney disease). Adult human serum K + The normal value range is 3.5-5.0 mmol/L, and the potassium contained in the blood is generally treated in China>5.0mmol/L was diagnosed as hyperkalemia. Hyperkalemia can induce various types of arrhythmia besides causing muscle twitching and paralysis, leads to sudden death in severe cases, and can increase the death risk of patients with chronic kidney diseases, heart failure, diabetes and complications. The chronic kidney disease is a serious disease which endangers the health of human bodies, and the prevalence rate of the chronic kidney disease reaches 11.7 to 15.1 percent globally. Clinically, the chronic kidney disease patient has the symptoms of renal function impairment, glomerular filtration rate reduction and K + Drainage is hindered and the risk of hyperkalemia is higher.
The good treatment effect of traditional Chinese medicine on chronic nephropathy shows unique advantages in clinical practice, and especially in the terminal stage of nephropathy patients, the traditional Chinese medicine decoction can improve malnutrition, calcium and phosphorus metabolism and micro inflammation of maintenance hemodialysis patients, improve the living quality of the patients and reduce complications. In early and middle stage renal failure patients, the traditional Chinese medicine decoction also has good clinical effect, and clinical contrast studies show that the kidney function of the patients can be obviously improved by adding the traditional Chinese medicine decoction. Zhanganning professor is a famous specialist for kidney diseases in China and makes an outstanding contribution to the research of kidney diseases for many years. Zhangdaling professor is the leading person in the department of nephropathy in our hospital, and Zhangzhong professor obtains obvious curative effect on chronic nephropathy by adopting traditional Chinese medicines. Kidney failure treating medicineModified Chenyixiao powder) is a common prescription for professor Zhangning to treat chronic kidney diseases, consists of astragalus root, rhizoma ligustici wallichii, salvia miltiorrhiza, oriental wormwood, trogopterus dung, cattail pollen charcoal, rhubarb charcoal and the like, and achieves obvious clinical curative effect on treating diseases such as chronic renal failure and the like. Clinical pharmacists find that the traditional Chinese medicine has the risk of causing hyperkalemia for patients with renal insufficiency in medication supervision of patients. Most of the Chinese medicinal materials belong to natural plant medicinal materials, K + High content, the water decoction method is more greatly used for decocting K in the medicinal materials + . Clinical K in renal patients + The intake is strictly limited, and the adult patient is advised to have K per day + The intake amount of (B) is 2000-2500mg (50-65 mmol). Therefore, taking traditional Chinese medicine decoction undoubtedly increases the K of patients + The intake amount of (A) for the renal disease patient K + The excretion of (A) causes a burden when K is in vivo + Above normal levels, complications of hyperkalemia may accompany. In patients with chronic kidney disease complicated with hyperkalemia, the risk of serious adverse cardiovascular events is greatly increased, and the survival rate of patients with chronic kidney disease is seriously influenced. Therefore, K contained in the Chinese medicinal decoction + Greatly limits the application of the medicine in patients with chronic kidney disease or hyperkalemia.
The most common measure currently taken clinically for reducing blood potassium levels is oral administration of K + Binding drugs by binding to K in the gastrointestinal tract + And promotion of K + Excreted thereby reducing blood potassium levels. But usually K + The adverse reaction of the gastrointestinal tract after the combined medicine is taken orally is not negligible, so that the compliance of the patient to take the medicine is reduced, and the use of the medicine by the patient with gastrointestinal tract diseases is limited. In addition, the potassium-lowering drugs all have adsorption effects, and other drugs taken together may have adsorption effects so as to influence the in vivo absorption of the drugs.
Disclosure of Invention
Aiming at the defects in the prior art, the invention designs and develops a traditional Chinese medicine decoction potassium removal process based on an ion exchange technology, and aims to remove potassium at different exchange temperatures and different exchange action times according to exchange resins with different qualities without preprocessing the resinsBy increasing K + Exchange rate and according to K in decoction + The concentration is used for estimating the exchange rate, thereby prejudging the potassium removal effect of the process.
The invention adopts the following technical scheme:
a process for removing potassium from the Chinese-medicinal decoction based on ion exchange technique includes adding exchange resin with different masses to the Chinese-medicinal decoction to be removed, and removing potassium at different exchange temperatures and different exchange times.
Furthermore, the dosage of the exchange resin is 0.5g to 3g of exchange resin added in every 30mL of decoction.
Furthermore, the dosage of the exchange resin is 2g of exchange resin added in every 30mL of decoction.
Further, the exchange resin is sodium polystyrene sulfonate.
Further, K is obtained after potassium removal exchange of the traditional Chinese medicine decoction to be subjected to potassium removal + An exchange rate W of
W＝10.302N 0.5056 (ii) a Wherein N = -26.37ln c-129.27, and c is initial K in the traditional Chinese medicine decoction to be subjected to potassium removal + And (4) concentration.
Further, the exchange temperature is 25-65 ℃.
Further, the exchange temperature was 25 ℃.
Further, the exchange time was 1 minute.
Further, in the potassium removal exchange, the agitation was carried out at a rate of 750rpm by stirring.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
the ion exchange technology-based traditional Chinese medicine decoction potassium removal process provided by the invention does not need to pretreat resin, and improves K by performing potassium removal application on exchange resins with different qualities at different exchange temperatures and different exchange action times + Exchange rate according to K in the Chinese medicinal decoction to be subjected to potassium removal + Initial concentration estimation K + Exchange rate, and further pre-judging the potassium removal effect of the traditional Chinese medicine decoction, thereby evaluating the necessity of carrying out potassium removal by using the process to realize reduction of potassium deficiencyThe purpose of the necessary losses.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention. The primary objects and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof.
Drawings
FIG. 1 is a Logk of the effect of temperature on resin in potassium reduction in the traditional Chinese medicine decoction potassium removal process d A schematic of the effect of the values;
FIG. 2 shows the temperature vs. resin in the process of removing potassium from the Chinese medicinal decoction according to the present invention versus Na in the decoction + A schematic of the effect of concentration;
FIG. 3 is a schematic diagram showing the influence of the stirring time on the potassium reduction effect of resin in the traditional Chinese medicine decoction potassium removal process;
FIG. 4 shows the mixing time of resin in the process for removing potassium from the Chinese medicinal decoction for adding Na in the decoction + A schematic of the effect of concentration;
FIG. 5 is a schematic diagram showing the effect of the resin dosage on the potassium reduction effect of the resin in the traditional Chinese medicine decoction potassium removal process;
FIG. 6 shows the resin dosage vs. Na in the Chinese medicinal decoction versus the resin in the process for removing potassium from the Chinese medicinal decoction according to the invention + A schematic of the effect of concentration;
FIG. 7 is a chromatogram of a mixed solution of standard substances of index components in the process of verifying the process of removing potassium from a decoction for treating renal failure by the process for removing potassium from a traditional Chinese medicine decoction;
FIG. 8 is a chromatogram of each component of a decoction to be tested in the process of verifying the process of removing potassium from a decoction for treating renal failure by the process of removing potassium from a traditional Chinese medicine decoction;
FIG. 9 shows three batches of samples K after potassium removal application is performed according to clinical dosage by the traditional Chinese medicine decoction potassium removal process + A schematic of the exchange rate;
FIG. 10 is a graph ofThe potassium removal process of the traditional Chinese medicine decoction is used for removing potassium according to clinical dosage of three batches of samples Na + Schematic of fold increase;
FIG. 11 shows K in clinical medication of different cases by the process for removing potassium from Chinese medicinal decoction + A schematic of the exchange rate;
FIG. 12 shows Na in the exchanged decoction of the traditional Chinese medicine decoction subjected to the potassium removal process in clinical medication of different cases + A schematic representation of the increase in the fold,
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The invention discloses a traditional Chinese medicine decoction potassium removal process based on an ion exchange technology, wherein exchange resins with different masses are added into a traditional Chinese medicine decoction to be subjected to potassium removal, and potassium removal exchange is carried out at different exchange temperatures and different exchange action times.
In another embodiment, the dosage of the exchange resin is 0.5g to 3g of exchange resin added in every 30mL of decoction; preferably, the amount of exchange resin is 2g per 30mL of decoction.
In another embodiment, the exchange resin is sodium polystyrene sulfonate.
In another embodiment, K is obtained after potassium removal exchange of the Chinese medicinal decoction to be subjected to potassium removal + An exchange rate W of
W＝10.302N 0.5056 (ii) a Wherein N = -26.37ln c-129.27, and c is initial K in the traditional Chinese medicine decoction to be subjected to potassium removal + And (4) concentration.
In another embodiment, the exchange temperature is from 25 ℃ to 65 ℃; in this embodiment, the exchange temperature is preferably 25 ℃.
In another embodiment, the exchange time is 1 minute.
In another embodiment, the potassium removal exchange is performed by stirring at a rate of 750rpm.
Example 1
1. Instrument and medicament
Raw astragalus membranaceus (batch No. 19092606, origin: the decoction pieces of Anhui cooperative and patent medicine, inc., chuan Xiong (lot 19090609, kyowa Pengzhou, anhui cooperative and patent medicine, inc., sichuan), danshen (lot 19120607, origin: ling city, anhui cooperative and patent medicine, inc., shandong province), artemisia capillaris (lot 1910010492, origin: shaanxi province, hu Zhen Yao medicine, inc., xianhui cooperative and patent medicine, inc.), vinegar trogopterus (lot 19110413, origin: shanxi province, lo city, anhui cooperative and patent medicine, inc.), cattail pollen charcoal (lot 19040802, origin: inner Mongolia Bazhuo Tuo, anhui cooperative and patent medicine, inc.), rhubarb charcoal (lot 19101507, origin: gansu province, anhui cooperative, anhui patent medicine, inc., poison Shuiye Shuiyun sodium, kangshui tablet, inc., polystyrol powder, shanghai Kangshui tablet, etc.).
7700X inductively coupled plasma Mass spectrometer (Agilent technologies, USA), one in ten thousand percent electronic analytical balance (stone Jiazhuang Wante instruments, inc. in Hebei province), AS62.R2 Ten ten thousand balance (Polish Duowei Inc.), MS300 heating magnetic stirrer (Shanghai Mustedt instruments, inc.), tenlin vortex mixer (Shanghai Damm industries, inc.), smart2Pure ultrapure water meter (Saimeishieshi technologies, china, inc.), electroceramic stove (Jiuyang, inc.), thermo Sorvall Legend Micro 21 microcentrifuge (Saimeishieshi, china, inc.), eppendorf liquid-moving gun (Ed.).
2. Preparation of renal failure traditional Chinese medicine decoction for removing potassium
Weighing 30g of raw astragalus membranaceus, 10g of ligusticum wallichii, 10g of salvia miltiorrhiza, 20g of oriental wormwood, 10g of trogopterus dung, 10g of cattail pollen charcoal and 20g of rhubarb charcoal according to the dose, placing the raw astragalus membranaceus, 10g of ligusticum wallichii, 10g of salvia miltiorrhiza, 20g of oriental wormwood, 10g of trogopterus dung, 10g of cattail pollen charcoal and 20g of rhubarb charcoal into an extraction container, soaking for 1h, heating with strong fire until the liquid is boiled, timing, heating with slow fire to keep the liquid surface slightly boiling, decocting for 60min, filtering the decoction while the decoction is hot, adding 6 times of water, heating with strong fire to boil, and decocting with slow fire for 50min, stopping heating, filtering while the decoction is hot, combining the two decoctions, appropriately concentrating if necessary, and combining the decoctions to obtain about 600mL of a decoction sample.
3. Step of potassium removal process
1. Metal ion detection
Accurately transferring 1mL of sample into a microwave digestion tank, adding 5mL of nitric acid, covering and placing for 1h, screwing a tank cover, and digesting according to the standard operation steps of a microwave digestion instrument. Cooling, taking out, slowly opening the tank cover, exhausting gas, washing the inner cover with a small amount of water, placing the digestion tank in an ultrasonic water bath tank, ultrasonically degassing for 2-5min, adding water to a constant volume of 50mL, mixing uniformly for later use, and simultaneously performing a blank test.
Inductively coupled plasma (ICP-MS) mass spectrometer parameters were set as follows: radio frequency power 1500W; the plasma gas flow is 15L/min; the carrier gas flow is 0.8L/min; the auxiliary gas flow is 0.4L/min; the flow rate of the helium gas is 4mL/min; the non-Wacker temperature is 2 ℃; the sample lifting rate is 0.3r/s; the sampling depth is 8mm; the number of repetitions was 3. The analysis mode is a collision reaction tank.
Accurately weighing 0.5mg of potassium chloride, dissolving, fixing the volume in a 100mL volumetric flask, uniformly mixing, and diluting step by step to obtain standard potassium chloride solutions with the concentrations of 0,0.1,0.25,0.5,1.0,2.5 and 5.0mg/L for later use.
Accurately weighing 0.5mg of sodium chloride, dissolving, diluting to constant volume in a 100mL volumetric flask, mixing uniformly, and diluting step by step to obtain standard sodium chloride solutions with the concentrations of 0,0.1,0.25,0.5,1.0,2.5 and 5.0mg/L for later use.
Determination of the Metal ions by the ICP-MS method, K + The standard curve equation of (1) is y =14.11x +3.535 (R =0.9999, range 0.1-5.0 mg/L); na (Na) + The standard curve equation of (1) is y =40.70x +1.841 (R =0.9999, range 0.1-5 mg/L).
K + The sample recovery rate is 95.4% of low concentration (1.0 mg/mL) and 100.9% of high concentration (2.5 mg/mL); na (Na) + The sample recovery rate was 96.2% at a low concentration (1.0 mg/mL) and 104.2% at a high concentration (2.5 mg/mL), respectively.
2. Adsorption of K to resin by action temperature + Influence of efficiency while suctionNa in the decoction before and after the attachment + Concentration monitoring
Accurately weighing 30mL of decoction sample, accurately weighing 2g of resin, washing the resin with ultrapure water for three times, and mixing with K in the decoction under magnetic stirring + Performing exchange, fixing the stirring speed at 750rpm, stirring for 1min, and performing exchange experiments at 25 deg.C, 35 deg.C, 45 deg.C, 55 deg.C, and 65 deg.C respectively; k + ICP-MS is adopted for concentration determination, and experimental results show that in the process of the action of the sodium polystyrene sulfonate resin on the traditional Chinese medicine decoction, along with the rise of temperature, the results are shown in figures 1 and 2, and logK d Has a reduced tendency but a smaller change, and compared with the decoction sample before resin action, na in the decoction after resin action + The concentration is obviously increased, and at the temperature of 25 ℃, na + The content increases by about 25 times, and Na in the decoction increases along with the increase of the action temperature + There is a downward trend.
3. Adsorption of K to resin with action time + Influence of efficiency, and simultaneous absorption of Na in the decoction before and after adsorption + Concentration monitoring
Accurately measuring 30mL decoction sample, accurately weighing 2g resin, cleaning the resin with ultrapure water for three times, and mixing with K in the decoction under magnetic stirring + Exchange is carried out, the fixed stirring speed is 750rpm, the fixed action temperature is 25 ℃, the action time is respectively set to be 1min,5min,10min,15min and 30min, and the K is measured by an ICP-MS method + The results are shown in FIG. 3 and FIG. 4, and the effect time is prolonged for K + The exchange rate has no obvious influence, and the prolonged action time does not affect Na in the decoction + Has a significant effect on the concentration of (c).
4. Resin dosage to resin adsorption K + Influence of efficiency, and simultaneous absorption of Na in the decoction before and after adsorption + Concentration monitoring
Setting the temperature at 25 deg.C, stirring at 750rpm for 1min, accurately weighing 0.5g, 1g, 1.5g, 2g, 2.5g, and 3g resin, respectively, exchanging with 30mL decoction of renal failure prescription, pretreating supernatant, and measuring K by ICP-MS + As shown in FIGS. 5 and 6, the concentration of K was increased as the amount of the resin used was increased + The rate of exchange is increased and,when the resin amount is increased to 2g, the exchange rate increase becomes smaller, and Na in the decoction increases with the resin amount + Also in an increasing trend.
Therefore, for K + The exchange influence of the formula (I) is the resin dosage, and the potassium removal process conditions in vitro established according to the renal failure formula decoction are that the K in the decoction is carried out according to the condition that 2g of resin is used for every 30mL of decoction, the temperature is 25 ℃, the action time is 1min + Is a suitable condition, in which process K + The exchange rate was 85.37% + -0.81%.
In this example, the sodium polystyrene sulfonate resin was screened for the influence factors (temperature, action time, resin dosage) of the ion exchange process in the renal failure decoction. The results show that the prolonged action time is applied to K in the decoction + Has no effect on the exchange of (2); increasing temperature of K in decoction + The exchange rate of (2) is decreased; the exchange capacity does not increase obviously after the resin dosage reaches 2g. Through the exchange test of small sample size, the optimal process for determining the renal failure decoction is as follows: 2g of resin is used per 30mL of decoction at 25 deg.C for 1min.
Example 2
Verification of potassium removal process of kidney failure formula decoction
1. Apparatus and medicine
<xnotran> ( 19092606, : , ), ( 19090609, : , ), ( 19120607, : , ), ( 1910010492, : , ), ( 19110413, : , ), ( 19040802, : , ), ( 19101507, : , ), ( ), ( , ), ( , ), ( , ), ( ≥ 98%, , : AF 20060608), ( ≥ 98%, , :110773 — 201915), B ( ≥ 98%, , : BWC 9040-2016), ( ≥ 98%, , : 110753-201817), -3-O- ( ≥ 98%, </xnotran> Shanghai-sourced leaf biotechnology limited, lot No.: Y17N9H 75485), typhaneoside (content not less than 98%, shanghai source leaf biotechnology limited, lot no: Y20A11H 116659)
7700X inductively coupled plasma Mass spectrometer (Agilent technologies, USA), wonth electronic analytical balance (Wonth instruments & Equipment Co., ltd., hebei province), AS62.R2 Ten-ten-thousandth balance (Polish Duowei Co., ltd.), MS300 heating magnetic stirrer (Shanghai instruments Co., ltd.), tenlin vortex mixer (Shanghai Du McFa), remag PXSJ-227L ion meter (Shanghai instruments electro scientific Co., ltd.), rt2 Smore ultra Pure water instrument (Sammer Feishi technologies, china Co., ltd.), decoction sand pan (Jiangxi Kangcera Co., ltd.), electroceramic stove (Jiuyang Gmby Co., ltd.), sorvall Legend 21 microcentrifuge ((Saifen Feishi technologies, china Co., ltd.)), eppendorf liquid-moving gun (Germany Bender Co., waters Uygur ultra-effective liquid chromatograph (Micro-LC science Co., ltd.))
2. Method and results
Accurately weighing calycosin glucoside, ferulic acid, salvianolic acid B, chlorogenic acid, isorhamnetin-3-O-neohesperidin and typhanoside standard substance 10mg respectively, dissolving in 50% methanol-water solution, transferring into a 10mL volumetric flask, fixing the volume, preparing into 1mg/mL mother liquor, and mixing well for later use.
After the mother solutions of the respective standard substances are mixed in equal amount, 50% methanol-water is added to dilute the mixture into mixed standard solutions with the concentrations of 0.0833,0.833,2.083,4.167,8.33, 12.5, 20.83 and 41.67 mu g/mL respectively for standby.
Respectively taking 1mL of decoction sample before and after ion exchange resin action, adding 50% methanol water solution to 10mL, mixing, centrifuging at 10000r/min for 15min, filtering supernatant with 0.22 μm microporous membrane, and detecting the filtrate on machine.
The Ultra Performance Liquid Chromatography (UPLC) conditions were: waters ACQUITY UPLC I-Class ultra high performance liquid chromatograph, ACQUITY UPLC CSH C18 column (1.7 μm, 2.1X 100 mm); mobile phase: 0.1% formic acid in water (A) -acetonitrile (B), gradient elution conditions: 0 → 4min:4% B,4 → 6min:4% → 13% B,6 → 12min:13% B,12 → 15min:13% → 20% B,15 → 20min:20% B,20 → 26min:20% → 26% B,26 → 28min:26% → 59% B,28 → 30min:50% → 65% B. Flow rate of mobile phase: 0.3mL/min; column temperature: 40 ℃; sample introduction volume: 2 mu L of the solution; detection wavelength: the chromatogram at 280nm is shown in FIGS. 7 and 8.
The accuracy of the method is measured by adopting the sample adding recovery rate, 9 sample solutions with the same volume and known sample concentration are respectively prepared, three standard substance mixed solutions with different concentrations, namely, low concentration 0.833 mu g/mL, medium concentration 8.33 mu g/mL and high concentration 41.67 mu g/mL, are added, and each concentration is parallelly divided into three parts to prepare 9 sample solutions with the same volume to be measured. The method has the advantages that the method has precision, and the same mixed standard solution is continuously injected for 6 times; the method has repeatability, wherein the decoction sample is parallelly processed by 6 samples in the same method, and is loaded on a machine for testing; the same sample is injected for 6 times at different times in one day for stability.
Taking the concentration of the compound to be measured as a horizontal coordinate and the peak area as a vertical coordinate, and adopting an external standard method to obtain a corresponding standard curve as follows: chlorogenic acid (y =7278.1x +318.14, R 2 =0.9995, range 0.0833-20.83 μ g/mL); ferulic acid (y =21444x +217.83, R 2 =0.9997, range 0.0833-20.83 μ g/mL); calycosin glucoside (y =15086x +110.2 2 =0.9995, range 0.0833-20.83 μ g/mL); typhaneoside (y =4137.1x-25.82 2 =0.9998, range 0.0833-20.83 μ g/mL); isorhamnetin-3-O-neohesperidin (y =4599.1x +440.83, R 2 =0.9995, range 0.0833-20.83 μ g/mL); salvianolic acid B (y =3063.9x-1373.2, R 2 =0.9992, range 0.0833-41.67 μ g/mL).
The accuracy, precision, repeatability and stability results of the method are shown in tables 1-4 respectively.
Table 1 method accuracy (n = 9)
TABLE 2 validation of method precision (n = 6)
Table 3 repeatability verification (n = 6)
Table 4 sample stability verification (n = 6)
Weighing 30g of raw astragalus, 10g of ligusticum wallichii, 10g of salvia miltiorrhiza, 20g of oriental wormwood, 10g of trogopterus dung, 10g of cattail pollen charcoal and 20g of rhubarb charcoal according to the dose, placing the raw astragalus, 10g of ligusticum wallichii, 10g of salvia miltiorrhiza, 20g of oriental wormwood, 10g of trogopterus dung, 10g of cattail pollen charcoal and 20g of rhubarb charcoal in an extraction container, adding 8 times of water into the extraction container, soaking for 1h, heating with strong fire until the liquid is boiled, timing, heating with slow fire until the liquid is boiled, keeping the liquid in a slightly boiling state, decocting for 60min, filtering the decoction while the decoction is hot, adding 6 times of water, heating with strong fire until the liquid is boiled, stopping heating after decocting with slow fire for 50min, filtering while the decoction is hot, combining the two decoctions, appropriately concentrating if necessary, combining the decoctions to obtain about 600mL of a decoction sample, and decocting three parts in parallel.
Per 30mL of the medicinal liquidThe dosage of 2g of resin is exchanged, and about 600mL of decoction is obtained in each dose, so about 40g of resin is used in each dose. Selecting the action temperature of 25 ℃ and the action time of 1min to carry out the potassium removal application of the resin. The results are shown in fig. 9 and 10, and the optimized action conditions are selected to carry out the resin potassium removal application according to the clinical dose, K + The exchange rate of (2) still reaches 80%.
The chromatogram of liquid phase detection of each component in the decoction is shown in fig. 7 and fig. 8, and the quantitative detection result is shown in table 5, the adsorption rate of the resin on chlorogenic acid is about 10.39% at least, the adsorption rate on isorhamnetin-3-O-neohesperidin is the highest, and reaches 86.59%, the adsorption rate on ferulic acid is 29.04%, the adsorption rate on salvianolic acid B is 18.13%, the adsorption rate on calycosin glucoside is 51.03%, and the adsorption rate on typhaneosin is 75.48%.
In the embodiment, the content of other components in the decoction before and after the potassium reduction effect is measured, and as shown in table 6, the minimum adsorption rate is about 14.95% and the maximum adsorption rate is 70.19% in 16 components.
TABLE 5 content change of 6 index components in decoction before and after potassium removal: (
n＝3)
TABLE 6 content change of 16 components in decoction before and after potassium removal: (
n＝3)
Example 3
1. Instrument and medicament
Prescription (No. 1): 40g of astragalus membranaceus, 20g of rhizoma smilacis glabrae, 10g of salvia miltiorrhiza, 10g of ligusticum wallichii, 10g of oriental wormwood, 10g of vinegar trogopterus dung, 10g of pollen typhae charcoal, 10g of vinegar turtle shell, 10g of vinegar tortoise shell, 10g of vinegar rhizoma sparganii, 10g of vinegar curcuma zedoary, 30g of dandelion, 20g of patrinia scabiosaefolia link, 20g of wine schisandra chinensis, 10g of rheum officinale, 20g of rheum officinale charcoal, 10g of fried endothelium corneum gigeriae galli, 10g of bran-fried fructus aurantii, 10g of angelica sinensis, 20g of sculellaria barbata, 10g of fructus amomi and 15g of poria cocos.
Prescription (No. 2): 60g of astragalus membranaceus, 10g of rhizoma smilacis glabrae, 10g of salvia miltiorrhiza, 20g of ligusticum wallichii, 20g of rhubarb charcoal, 10g of cattail pollen charcoal, 10g of oriental wormwood, 20g of patrinia scabiosaefolia, 20g of vinegar turtle shell, 10g of fructus amomi, 20g of salt fructus psoraleae, 10g of cinnamon, 10g of dried orange peel, 20g of sculellaria barbata, 20g of wine schisandra chinensis, 10g of bran-fried fructus aurantii, 20g of exocarpium benincasae, 10g of vinegar rhizoma zedoariae, 10g of vinegar rhizoma sparganii, 20g of bran-fried rhizoma atractylodis macrocephalae, 30g of dandelion, 10g of salt eucommia ulmoides, 20g of oldenlandia diffusa and 10g of fried endothelium corneum gigeriae galli.
Prescription (No. 3): 40g of astragalus membranaceus, 10g of glabrous greenbrier rhizome, 10g of ligusticum wallichii, 10g of salvia miltiorrhiza, 10g of oriental wormwood, 10g of vinegar-processed trogopterus dung, 10g of cattail pollen charcoal, 10g of wine-processed schisandra chinensis, 20g of wine-processed glossy privet fruit, 20g of eclipta, 10g of dried dendrobium, 10g of radix pseudostellariae, 10g of polygonum aviculare, 10g of fructus amomi, 10g of vinegar-processed tortoise shell, 10g of vinegar-processed turtle shell, 6g of liquorice tablets, 10g of poria cocos, 15g of radix bupleuri, 10g of scutellaria baicalensis tablets, 10g of clear water pinellia ternate and 10g of honey-fried licorice root.
Prescription (No. 4): 60g of astragalus membranaceus, 10g of rhizoma smilacis glabrae, 10g of salvia miltiorrhiza, 20g of ligusticum wallichii, 20g of patrinia scabiosaefolia, 20g of carbonized rhubarb, 10g of carbonized pollen typhae, 10g of rheum officinale, 10g of raspberry, 15g of wine-processed schisandra chinensis, 20g of calcined oyster, 10g of dried orange peel, 15g of bran-fried fructus aurantii, 15g of bighead atractylodes rhizome, 10g of earthworm, 15g of red paeony root, 30g of exocarpium benincasae, 15g of fried chicken's gizzard-membrane, 15g of gastrodia elata, 15g of vinegar-processed turtle shell, 20g of flatstem milkvetch seed and 20g of bran-fried gorgon fruit.
Prescription (No. 5): 60g of astragalus membranaceus, 20g of rhizoma smilacis glabrae, 30g of ligusticum wallichii, 30g of radix paeoniae rubra, 10g of vinegar curcuma zedoary, 20g of bran-fried fructus aurantii, 10g of vinegar turtle shell, 15g of sculellaria barbata, 10g of wine-processed schisandra chinensis, 20g of raspberry, 15g of fried chicken's gizzard-membrane, 10g of dried orange peel, 15g of rhubarb charcoal, 15g of pollen typhae charcoal, 20g of fried spina date seed, 30g of herba patriniae, 15g of angelica sinensis and 15g of radix paeoniae alba.
Prescription (No. 6): 50g of astragalus membranaceus, 10g of rhizoma smilacis glabrae, 20g of salvia miltiorrhiza, 15g of ligusticum wallichii, 20g of rhubarb charcoal, 10g of cattail pollen charcoal, 10g of oriental wormwood, 30g of patrinia scabiosaefolia, 20g of vinegar turtle shell, 10g of fructus amomi, 20g of salt fructus psoraleae, 10g of cinnamon, 20g of sculellaria barbata, 20g of wine-processed schisandra chinensis, 20g of bran-fried fructus aurantii, 10g of vinegar curcuma zedoary, 10g of vinegar rhizoma sparganii, 15g of fried chicken's gizzard-membrane, 20g of achyranthes bidentata, 30g of exocarpium benincasae, 10g of rheum officinale, 20g of bighead atractylodes rhizome and 20g of angelica sinensis.
Prescription (No. 7): 60g of astragalus membranaceus, 10g of rhizoma smilacis glabrae, 15g of salvia miltiorrhiza, 20g of ligusticum wallichii, 15g of fructus aurantii immaturus stir-fried with bran, 15g of wine-processed schisandra chinensis, 15g of raspberry, 20g of gordon euryale seed stir-fried with bran, 10g of vinegar-processed curcuma zedoary, 30g of rhizoma dioscoreae septemlobae, 30g of patrinia scabiosaefolia, 10g of oriental wormwood, 30g of rhubarb charcoal, 10g of pollen typhae charcoal, 20g of vinegar-processed turtle shell, 15g of calcined oyster, 20g of cherokee rose pulp, 10g of fructus amomi, 20g of sculellaria barbata and 15g of bighead atractylodes rhizome stir-fried with bran.
Prescription (No. 8): 60g of astragalus membranaceus, 15g of rhizoma smilacis glabrae, 20g of ligusticum wallichii, 30g of rhubarb charcoal, 10g of pollen typhae charcoal, 10g of lumbricus, 10g of fried stiff silkworm, 10g of cassia twig, 20g of herba patriniae, 20g of desmodium, 10g of radix achyranthis bidentatae, 30g of honey mulberry bark, 15g of calcined oyster shell, 15g of vinegar rhizoma sparganii, 20g of bran-fried fructus aurantii, 15g of radix pseudostellariae, 15g of wine-processed fructus schizandrae, 10g of oriental wormwood, 15g of raspberry and 15g of angelica sinensis.
Prescription (No. 9): 30g of astragalus membranaceus, 30g of wine-processed schisandra chinensis, 20g of dandelion, 20g of patrinia scabiosaefolia, 20g of oriental wormwood, 20g of vinegar-processed trogopterus dung, 20g of pollen typhae charcoal, 10g of rheum officinale, 20g of rheum officinale charcoal, 10g of winged euonymus twig, 10g of polygonum aviculare, 10g of fringed pink, 20g of sculellaria barbata, 10g of salvia miltiorrhiza, 10g of ligusticum wallichii, 10g of vinegar-processed rhizoma sparganii, 10g of vinegar-processed curcuma zedoary, 20g of bran-fried fructus aurantii, 10g of angelica sinensis and 10g of wine-processed radix paeoniae alba.
Prescription (No. 10): 60g of astragalus membranaceus, 15g of rhizoma smilacis glabrae, 10g of salvia miltiorrhiza, 30g of ligusticum wallichii, 10g of rheum officinale, 15g of rhubarb charcoal, 5g of vinegar-processed trogopterus dung, 5g of pollen typhae charcoal, 15g of oriental wormwood, 30g of radix puerariae, 30g of wine-processed cornus officinalis, 10g of fructus amomi, 3g of scalded leech, 15g of wine-processed schisandra chinensis, 30g of exocarpium benincasae, 15g of dandelion, 15g of sculellaria barbata, 15g of cherokee rose fruit, 20g of keel and 10g of albizia flower.
7700X inductively coupled plasma mass spectrometer (Agilent technologies, USA), one in ten thousand percent electronic analytical balance (Maskyu Wante instruments, inc., hebei province), AS62.R2 one in ten thousand balance (Polish Dowei Inc.), MS300 heated magnetic stirrer (Shanghai Mustett instruments, inc.), tenlin vortex mixer (Shangham Musteur industries, inc.), smart2Pure ultrapure water meter (Sammer Feishell technologies, inc.), electroceramic stove (Jiu Yang GmbH), thermo Sorvall Legend Micro 21 microcentrifuge (Sammer Feishell technologies, china, inc.), eppendorf liquid transfer gun (Elegend, germany), polystyrene sodium powder (Shanghai Kangshi pharmaceuticals, inc.).
2. Preparation of renal failure traditional Chinese medicine decoction for removing potassium
Weighing the traditional Chinese medicines according to the prescription dose (No. 1-No. 10) respectively, placing the traditional Chinese medicines into an extraction container, adding 8 times of water, soaking for 1h, heating with strong fire until the liquid is boiled, timing, heating with slow fire to keep the liquid surface in a slightly boiling state, decocting for 60min, filtering the decoction while hot, adding 6 times of water, heating with strong fire until the liquid is boiled, decocting with slow fire for 50min, stopping heating, filtering while hot, combining the two decoctions, concentrating properly if necessary, and combining the decoctions to obtain about 600mL of a decoction sample.
3. Calculating K + Exchange rate
Exchanging according to the dosage of 2g resin per 30mL liquid medicine to obtain 600mL decoction liquid per medicine, so that 40g resin is used per medicine, selecting the action temperature of 25 ℃ and the action time of 1min, selecting the optimized action condition, and performing resin potassium removal application according to clinical dosage, wherein the result is shown in figure 11 + The removal rate exceeds 60%, the maximum value reaches 80.3%, the minimum value reaches 62.5%, and after resin action, as shown in figure 12, na + All have obvious increase, the maximum increase is 20.6 times, the minimum increase is 6.4 times, and the initial K in the traditional Chinese medicine decoction to be subjected to potassium removal is determined according to an ICP-MS method before the application of potassium removal + After concentration, W =10.302N 0.5056 (ii) a Wherein, N = -26.37ln c-129.27, c is initial K in the traditional Chinese medicine decoction to be subjected to potassium removal + The concentration (unit mol/L) and K after potassium removal application are measured according to an ICP-MS method + Content, calculating the actual K + The exchange rate and the obtained data are shown in Table 7, and it can be seen that the potassium removal process provided by the invention is simultaneously carried out according to K in the traditional Chinese medicine decoction to be subjected to potassium removal + Initial concentration estimate K + The exchange rate and the potassium removal effect of the traditional Chinese medicine decoction are predicted, so that the necessity of removing potassium by using the process is evaluated, the experimental efficiency is improved, unnecessary loss is reduced, and further moreThe clinical application is good.
TABLE 7K + Exchange rate
The invention establishes the in vitro removal of K in the traditional Chinese medicine decoction of the sodium polystyrene sulfonate + The method can well remove K in the liquid medicine by optimizing and verifying the process + The invention provides data support for the later application of the invention to clinical practice and provides pharmaceutical technical services for ensuring the safe application of traditional Chinese medicines and ensuring safe medication of CKD (CKD) patients with hyperkalemia and dangerous people with hyperkalemia.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that may be considered by those skilled in the art within the technical scope of the present invention disclosed herein should be covered within the scope of the present invention.
Claims (9)
1. A traditional Chinese medicine decoction potassium removal process based on an ion exchange technology is characterized in that exchange resins with different qualities are added into a traditional Chinese medicine decoction to be subjected to potassium removal, and potassium removal exchange is carried out at different exchange temperatures and different exchange action times.
2. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 1, wherein the dosage of the exchange resin is 0.5 g-3 g of the exchange resin added in each 30mL of the decoction.
3. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 2, wherein the dosage of the exchange resin is 2g per 30mL of the decoction.
4. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process according to claim 2 or 3, wherein the exchange resin is sodium polystyrene sulfonate.
5. The ion exchange technology-based potassium ion exchange rate W of the traditional Chinese medicine decoction to be subjected to potassium removal exchange in claim 4 is
W＝10.302N 0.5056 (ii) a Wherein, N = -26.37lnc-129.27, and c is the initial potassium ion concentration in the traditional Chinese medicine decoction to be subjected to potassium removal.
6. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 5, wherein the exchange temperature is 25-65 ℃.
7. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 6, wherein the exchange temperature is 25 ℃.
8. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 6, wherein the exchange action time is 1 minute.
9. The ion exchange technology-based traditional Chinese medicine decoction potassium removal process of claim 6, wherein the potassium removal exchange is carried out by stirring at a stirring speed of 750rpm.
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